反应详情
EQUATION
反应方程式
REACTANTS
反应物
PRODUCTS
生成物
AUXILIARIES
试剂、催化剂与溶剂
PROCEDURE
实验过程
Sodium (0.5 g, 22 mmol) was added to anhydrous ethanol (50 ml) under nitrogen. When all of the sodium had reacted, 2-amino-6-chloropurine (750 mg, 4.42 mmol) was added. The reaction was refluxed for 3 h. After cooling, the reaction mixture was neutralised with glacial acetic acid and the solvent was removed. Recrystallisation from water gave the product as a white solid (548 mg, 69%), m.p.>230° C.; (Found: C, 46.76; H, 4.97; N, 39.09. Calc. for C7H9N5O: C, 46.92; H, 5.06; N, 39.09%); νmax (cm−1) 3505, 3484, 3432, 3324, 3191, 3110, 2984, 2901, 2705, 2544 (NH, C—H, NH2); δH (200 MHz, d6-DMSO) 7.808 (1H, s, C(8)H), 6.224 (2H, s, NH2), 4.437 (2H, q, J=7.1 Hz, OCH2), 1.353 (3H, t, J=7.1 Hz. CH2CH3); m/z 179 (M+, 100%), 169 (19), 164 (35), 151 ([MH—Et]+, 36%), 135 ([MH—OEt]+, 43%), 131 (38), 119 (34), 109 (54), 81 (41), 69 (39), 60 (21), 55 (31), 41 (48),
WORKUP
后处理
- temperatureThe reaction was refluxed for 3 h
- temperatureAfter cooling
- customthe solvent was removed
- customRecrystallisation from water